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Water → HCID 22504378, 화합물

HRID 1814116
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HRID 1814116 반응식
[CH2:1]([O:3][C:4]([C:6]1[O:7][C:8]([C:11]#[C:12][Si](C)(C)C)=[CH:9][CH:10]=1)=[O:5])[CH3:2].C1(S([NH:26][C:27]2[C:32](I)=[CH:31][C:30]([S:34]([CH3:37])(=[O:36])=[O:35])=[CH:29][CH:28]=2)(=O)=O)C=CC=CC=1.C([O-])(=O)C.[K+].O>CN(C)C=O>[CH2:1]([O:3][C:4]([C:6]1[O:7][C:8]([C:11]2[NH:26][C:27]3[C:28]([CH:12]=2)=[CH:29][C:30]([S:34]([CH3:37])(=[O:36])=[O:35])=[CH:31][CH:32]=3)=[CH:9][CH:10]=1)=[O:5])[CH3:2]
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참가 물질

6

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HCID 962WaterHCID 517044Potassium AcetateHCID 22504370HCID 22504370, 화합물HCID 225043761-Benzenesulfonylamino-2-iodo-4-methanesulfonylbenzene

생성물 1

HCID 22504378HCID 22504378, 화합물수율 65.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

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온도
100 °C

실험 절차

To a solution of the compound obtained in Example 29 (2) (0.1 g) in N,N-dimethylformamide (1 ml), 2-benzenesulfonylamino-3-iodo-5-methanesulfonylbenzene (0.0925 g), bistriphenylphosphine palladium dichloride (0.015 g), cuprous iodide (0.004 g) and potassium acetate (0.04 g) were added successively and the mixture was stirred in a sealed tube at 100° C. for 2 hours. After cooling, the reaction solution was poured into water, extracted with ethyl acetate, washed with a saturated aqueous NaCl solution, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The resulting residue was separated using silica gel column chromatography (hexane:ethyl acetate=1:1) to obtain 0.0462 g of the desired product as a brown solid.

후처리

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. washwashed with a saturated aqueous NaCl solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe resulting residue was separated

출처 및 근거

ORD 기록
ord-ddd3e2552b0e4a2f8a60e6edbd4595ef
출처 데이터셋
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06875770B2

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